Development and validation of a multi-residue and multi-class screening method of 44 antibiotics in salmon (Salmo salar) using ultra-high-performance liquid chromatography/time-of-flight mass spectrometry: Application to farmed salmon.

Affiliation

REQUIMTE/LAQV, Pharmacy Faculty, University of Coimbra, Azinhaga de Santa Comba, 3000-548 Coimbra, Portugal. Electronic address: [Email]

Abstract

A fast and sensitive multi-residue and multiclass screening method for the simultaneous determination of 44 antimicrobials in salmon muscle, using ultra- high-performance liquid chromatography/time-of-flight mass spectrometry (UHPLC-TOF/MS), was develop and validated. Two different procedures for the extraction step were tested, and an extraction with acetonitrile, ethylenediaminetetra acetic acid (EDTA) and n-hexane proved to be the best alternative. The method was validated, in accordance with Decision 2002/657/EC, using a qualitative approach at the CCβ level. The detection of the analytes was accomplished by retention time and accurate mass, whose maximum error should not exceed 5 ppm. All the compounds were successfully detected and identified at concentration levels corresponding to ½ maximum residue limit (MRL). The screening method was applied to 39 store bought samples of farmed salmon purchased in Portugal, originating from Norway and Denmark, and no antibiotic residues were detected.

Keywords

Antibiotics,Qualitative validation,Salmon,Screening,UHPLC-TOF/MS,

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